HRID249664

反应详情

EQUATION

反应方程式

HRID 249664 的结构方程式

PROCEDURE

实验过程

To a solution of 6-amino-5-chloro-2-(4-chlorophenyl)-4-pyrimidinecarboxylic acid (i.e. the product of Example 4, Step C) (20.0 g, 70.4 mmol) in ethanol (70 mL) was added thionyl chloride (5.14 mL, 70.4 mmol) while maintaining the temperature below 15° C. using an ice bath. The reaction mixture was then heated at reflux overnight. Water was added. Then with external cooling aqueous sodium hydroxide (50%) was added to adjust the pH to 7. The resulting solid was isolated by filtration and dried to afford the title product, a compound of the present invention, as a light beige solid (20.1 g).

WORKUP

后处理

  1. temperaturewhile maintaining the temperature below 15° C.
  2. temperatureThe reaction mixture was then heated
  3. temperatureat reflux overnight
  4. customThe resulting solid was isolated by filtration
  5. customdried